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Nanomaterials Applied to Analytical Chemistry

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A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Applied Chemistry".

Deadline for manuscript submissions: closed (28 February 2023) | Viewed by 21897

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Dr. Javier Hernández-Borges

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Guest Editor

Departamento de Química, Unidad Departamental de Química Analítica, Facultad de Ciencias, Universidad de La Laguna (ULL), Avda. Astrofísico Francisco Sánchez, s/n°, 38206 San Cristóbal de La Laguna, Spain
Interests: analytical chemistry; microplastics; environmental analysis; organic contaminants; sample preparation; chromatographic techniques; mass spectrometry

Dr. Javier González-Sálamo

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Co-Guest Editor

Special Issue Information

Dear Colleagues,

Nanoscience and nanotechnology, which produce materials for their applications well below the submicroscopic level (<100 nm), have reached an extraordinary level of development. At the nm level, surface physics and chemistry start to dominate the material’s properties. If such a fact is properly considered and managed, it can be of high utility in different disciplines.

In the case of Analytical Chemistry, nanomaterials occupy an important place in current research, especially in sample preparation procedures. Proof of this is the extremely high number of publications that appear each year that broaden more and more the applications and utilities of these materials with unique properties.

This Special Issue intends to compile recent and novel application of nanomaterials (metal–organic frameworks, covalent–organic frameworks, magnetic or nonmagnetic coated and noncoated nanoparticles, carbon-based nanomaterials such as carbon nanotubes, nanohorns, graphene, fullerenes, and others, etc.) in sample preparation procedures. Applications of nanomaterials in solid-phase extraction (SPE), including its dispersive (dSPE) or conventional mode as well as its miniaturized (µSPE, pipette tip SPE, etc.) or magnetic versions (m-dSPE, m-µdSPE, etc.), in solid-phase microextraction (SPME), matrix solid-phase dispersion (MSPD), stir bar (SBSE) or stir cake (SCSE) sorptive extraction, among others, and their combinations with liquid-phase extraction procedures, are highly welcome as well as review articles.

I hope you will find this Special Issue of interest. Your contribution will absolutely promote its success.

Sincerely yours,

Prof. Dr. Javier Hernández-Borges
Dr. Javier González-Sálamo
Guest Editors

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Keywords

Carbon-based nanomaterials
Quantum dots
Metal–organic frameworks
Covalent–organic frameworks
Coated and noncoated nanoparticles
Sorbent-based extraction techniques
Miniaturized extraction procedures

Published Papers (10 papers)

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Research

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12 pages, 4354 KiB

Open AccessArticle

Dispersive Micro-Solid Phase Extraction Using a Graphene Oxide Nanosheet with Neocuproine and Batocuproine for the Preconcentration of Traces of Metal Ions in Food Samples

by Barbara Feist

Molecules 2023, 28(10), 4140; https://doi.org/10.3390/molecules28104140 - 17 May 2023

Cited by 3 | Viewed by 996

Abstract

A dispersive micro-solid phase extraction (Dµ-SPE) method for the preconcentration of trace metal ions (Pb, Cd, Cr, Mn, Fe, Co, Ni, Cu, Zn) on graphene oxide with the complexing reagents neocuproine or batocuproine is presented here. Metal ions form cationic complexes with neocuproine and batocuproine. These compounds are adsorbed on the GO surface via electrostatic interactions. The factors affecting the separation and preconcentration of analytes such as pH, eluent (concentration, type, volume), amount of neocuproine, batocuproine and GO, mixing time, and sample volume were optimized. The optimal sorption pH was 8. The adsorbed ions were effectively eluted with 5 mL 0.5 mol L⁻¹ HNO₃ solution and determined by the ICP-OES technique. The preconcentration factor for the GO/neocuproine and GO/batocuproine in the range 10–100 and 40–200 was obtained for the analytes, with detection limits of 0.035–0.84 ng mL⁻¹ and 0.047–0.54 ng mL⁻¹, respectively. The method was validated by the analysis of the three certified reference materials: M-3 HerTis, M-4 CormTis, and M-5 CodTis. The procedure was applied to determine metal levels in food samples. Full article

(This article belongs to the Special Issue Nanomaterials Applied to Analytical Chemistry)

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16 pages, 5312 KiB

Open AccessArticle

Fe–Decorated Nitrogen–Doped Carbon Nanospheres as an Electrochemical Sensing Platform for the Detection of Acetaminophen

by Xiangchuan Zhao, Liping Zhang, Zhaoyun Chu, Qing Wang, Yue Cao, Jun Cao, Jiao Li, Wu Lei, Boming Zhang and Weimeng Si

Molecules 2023, 28(7), 3006; https://doi.org/10.3390/molecules28073006 - 28 Mar 2023

Cited by 6 | Viewed by 1571

Abstract

In this work, Fe–decorated nitrogen–doped carbon nanospheres are prepared for electrochemical monitoring of acetaminophen. Via a direct pyrolysis of the melamine–formaldehyde resin spheres, the well–distributed Fe–NC spheres were obtained. The as–prepared Fe–NC possesses enhanced catalysis towards the redox of acetaminophen for abundant active sites and high–speed charge transfer. The effect of loading Fe species on the electrochemical sensing of acetaminophen is investigated in detail. The synergistic effect of nitrogen doping along with the above–mentioned properties is taken advantage of in the fabrication of electrochemical sensors for the acetaminophen determination. Based on the calibration plot, the limits of detection (LOD) were calculated to be 0.026 μM with a linear range from 0–100 μM. Additionally satisfactory repeatability, stability, and selectivity are obtained. Full article

(This article belongs to the Special Issue Nanomaterials Applied to Analytical Chemistry)

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15 pages, 5458 KiB

Open AccessArticle

Enhancing Electrochemical Performance with g-C₃N₄/CeO₂ Binary Electrode Material

by M. Chandra Sekhar, Nadavala Siva Kumar, Mohammad Asif, Surya Veerendra Prabhakar Vattikuti and Jaesool Shim

Molecules 2023, 28(6), 2489; https://doi.org/10.3390/molecules28062489 - 08 Mar 2023

Cited by 6 | Viewed by 1483

Abstract

An innovative form of 2D/0D g-C₃N₄/CeO₂ nanostructure was synthesized using a simple precursor decomposition process. The 2D g-C₃N₄ directs the growth of 0D CeO₂ quantum dots, while also promoting good dispersion of CeO₂QDs. This 2D/0D nanostructure shows a capacitance of 202.5 F/g and notable rate capability and stability, outperforming the g-C₃N₄ electrode, reflecting the state-of-the-art g-C₃N₄ binary electrodes. The binary combination of materials also enables an asymmetric device (g-C₃N₄/CeO₂QDs//AC) to deliver the highest energy density (9.25 Wh/kg) and power density (900 W/kg). The superior rate capacity and stability endorsed the quantum structural merits of CeO₂QDs and layered g-C₃N₄, which offer more accessible sites for ion transport. These results suggest that the g-C₃N₄/CeO₂QDs nanostructure is a promising electrode material for energy storage devices. Full article

(This article belongs to the Special Issue Nanomaterials Applied to Analytical Chemistry)

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16 pages, 3681 KiB

Open AccessArticle

Effective Removal of Sulfonamides Using Recyclable MXene-Decorated Bismuth Ferrite Nanocomposites Prepared via Hydrothermal Method

by Pascaline Sanga, Juanjuan Wang, Xin Li, Jia Chen and Hongdeng Qiu

Molecules 2023, 28(4), 1541; https://doi.org/10.3390/molecules28041541 - 05 Feb 2023

Cited by 10 | Viewed by 1764

Abstract

Developing a simple and efficient method for removing organic micropollutants from aqueous systems is crucial. The present study describes the preparation and application, for the first time, of novel MXene-decorated bismuth ferrite nanocomposites (BiFeO₃/MXene) for the removal of six sulfonamides including sulfadiazine (SDZ), sulfathiazole (STZ), sulfamerazine (SMZ), sulfamethazine (SMTZ), sulfamethoxazole (SMXZ) and sulfisoxazole (SXZ). The properties of BiFeO₃/MXene are enhanced by the presence of BiFeO₃ nanoparticles, which provide a large surface area to facilitate the removal of sulfonamides. More importantly, BiFeO₃/MXene composites demonstrated remarkable sulfonamide adsorption capabilities compared to pristine MXene, which is due to the synergistic effect between BiFeO₃ and MXene. The kinetics and isotherm models of sulfonamide adsorption on BiFeO₃/MXene are consistent with a pseudo-second-order kinetics and Langmuir model. BiFeO₃/MXene had appreciable reusability after five adsorption–desorption cycles. Furthermore, BiFeO₃/MXene is stable and retains its original properties upon desorption. The present work provides an effective method for eliminating sulfonamides from water by exploiting the excellent texture properties of BiFeO₃/MXene. Full article

(This article belongs to the Special Issue Nanomaterials Applied to Analytical Chemistry)

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11 pages, 2952 KiB

Open AccessFeature PaperArticle

Assembly-Induced Emission Enhancement in Glutathione-Capped Bimetallic Gold and Copper Nanoclusters by Al³⁺ Ions and Further Application in Myricetin Determination

by Hao-Jie Bai, De-Yan Qi, Hong-Wei Li and Yuqing Wu

Molecules 2023, 28(2), 758; https://doi.org/10.3390/molecules28020758 - 12 Jan 2023

Cited by 1 | Viewed by 1361

Abstract

A significant emission enhancement (>100-fold) of glutathione-capped bimetallic gold and copper nanoclusters (AuCuNC@GSH) was achieved by assembling with Al³⁺ ions and by assembly-induced emission enhancement (AIEE). Further chelation of myricetin to Al³⁺ resulted in emission quenching of AuCuNC-Al³⁺, which was applied to specifically detect myricetin. Two linear responses were shown in the range of 0–1.5 μM and 1.5–50 μM, separately, leading to a low limit of detection at 8.7 nM. The method was successfully and accurately applied to myricetin determination in grape juice, which showed good application for real samples. Finally, the in-depth mechanism revealed that both the chelation of myricetin and Al³⁺ and the inner filter effect (IFE) between myricetin-Al³⁺ and AuCuNC-Al³⁺ greatly contributed to the quenching response of myricetin. Therefore, the present study provides an easy way to improve the fluorescence property of metal nanoclusters. Additionally, it supplies a cost-effective and easily performed approach to detect myricetin with high selectivity and sensitivity. Full article

(This article belongs to the Special Issue Nanomaterials Applied to Analytical Chemistry)

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16 pages, 6328 KiB

Open AccessArticle

Efficient Adsorption and Extraction of Glutathione S-Transferases with Glutathione-Functionalized Graphene Oxide–Polyhedral Oligomeric Silsesquioxane Composite

by Jingqi Sun, Limin Jia and Xuwei Chen

Molecules 2023, 28(1), 340; https://doi.org/10.3390/molecules28010340 - 01 Jan 2023

Cited by 1 | Viewed by 1451

Abstract

Glutathione S-transferases (GSTs) are important type-II detoxification enzymes that protect DNA and proteins from damage and are often used as protein tags for the expression of fusion proteins. In the present work, octa-aminopropyl caged polyhedral oligomeric silsesquioxane (OA–POSS) was prepared via acid-catalyzed hydrolysis of 3-aminopropyltriethoxysilane and polymerized on the surface of graphene oxide (GO) through an amidation reaction. Glutathione (GSH) was then modified to GO–POSS through a Michael addition reaction to obtain a GSH-functionalized GO–POSS composite (GPG). The structure and characteristics of the as-prepared GPG composite were characterized using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), thermogravity analysis, and surface charge analysis. The specific binding interactions between glutathione and GST gave GPG favorable adsorption selectivity towards GST, and other proteins did not affect GST adsorption. The adsorption behavior of GST on the GPG composite conformed to the Langmuir isotherm model, and the adsorption capacity of GST was high up to 364.94 mg g⁻¹ under optimal conditions. The GPG-based solid-phase adsorption process was applied to the extraction of GST from a crude enzyme solution of pig liver, and high-purity GST was obtained via SDS-PAGE identification. Full article

(This article belongs to the Special Issue Nanomaterials Applied to Analytical Chemistry)

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14 pages, 1031 KiB

Open AccessArticle

Determination of Hg(II) and Methylmercury by Electrothermal Atomic Absorption Spectrometry after Dispersive Solid-Phase Microextraction with a Graphene Oxide Magnetic Material

by Yesica Vicente-Martínez, María Jose Muñoz-Sandoval, Manuel Hernandez-Cordoba and Ignacio Lopez-Garcia

Molecules 2023, 28(1), 14; https://doi.org/10.3390/molecules28010014 - 20 Dec 2022

Cited by 1 | Viewed by 1636

Abstract

The toxicity of all species of mercury makes it necessary to implement analytical procedures capable of quantifying the different forms this element presents in the environment, even at very low concentrations. In addition, due to the assorted environmental and health consequences caused by each mercury species, it is desirable that the procedures are able to distinguish these forms. In nature, mercury is mainly found as Hg⁰, Hg²⁺ and methylmercury (MeHg), with the latter being rapidly assimilated by living organisms in the aquatic environment and biomagnified through the food chain. In this work, a dispersive solid-phase microextraction of Hg²⁺ and MeHg is proposed using as the adsorbent a magnetic hybrid material formed by graphene oxide and ferrite (Fe₃O₄@GO), along with a subsequent determination by electrothermal atomic absorption spectrometry (ETAAS). On the one hand, when dithizone at a pH = 5 is used as an auxiliary agent, both Hg(II) and MeHg are retained on the adsorbent. Next, for the determination of both species, the solid collected by the means of a magnet is suspended in a mixture of 50 µL of HNO₃ (8% v/v) and 50 µL of H₂O₂ at 30% v/v by heating for 10 min in an ultrasound thermostatic bath at 80 °C. On the other hand, when the sample is set at a pH = 9, Hg(II) and MeHg are also retained, but if the solid collected is washed with N-acetyl-L-cysteine only, then the Hg(II) remains on the adsorbent, and can be determined as indicated above. The proposed procedure exhibits an enrichment factor of 49 and the determination presents a linear range between 0.1 and 10 µg L⁻¹ of mercury. The procedure has been applied to the determination of mercury in water samples from different sources. Full article

(This article belongs to the Special Issue Nanomaterials Applied to Analytical Chemistry)

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12 pages, 1826 KiB

Open AccessArticle

Kinetic Analysis of Prostate-Specific Antigen Interaction with Monoclonal Antibodies for Development of a Magnetic Immunoassay Based on Nontransparent Fiber Structures

by Alexey V. Orlov, Alexandr G. Burenin, Artemiy M. Skirda and Petr I. Nikitin

Molecules 2022, 27(22), 8077; https://doi.org/10.3390/molecules27228077 - 21 Nov 2022

Cited by 5 | Viewed by 1667

Abstract

Prostate cancer is the second most common cancer diagnosed in men worldwide. Measuring the prostate-specific antigen (PSA) is regarded as essential during prostate cancer screening. Early diagnosis of this disease relapse after radical prostatectomy requires extremely sensitive methods. This research presents an approach to development of an ultrasensitive magnetic sandwich immunoassay, which demonstrates the limit of PSA detection in human serum of 19 pg/mL at a dynamic range exceeding 3.5 orders of concentration. Such attractive performance stems, inter alia, from the kinetic analysis of monoclonal antibodies (mAbs) against free PSA to select the mAbs exhibiting best kinetic characteristics and specificity. The analysis is carried out with a label-free multiplex spectral-correlation interferometry compatible with inexpensive single-use glass sensor chips. The high sensitivity of developed PSA immunoassay is due to electronic quantification of magnetic nanolabels functionalized by the selected mAbs and three-dimension porous filters used as an extended solid phase. The assay is promising for PSA monitoring after radical prostatectomy. The proposed versatile approach can be applied for the rational design of highly sensitive tests for detection of other analytes in many fields, including in vitro diagnostics, veterinary, food safety, etc. Full article

(This article belongs to the Special Issue Nanomaterials Applied to Analytical Chemistry)

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11 pages, 2277 KiB

Open AccessArticle

Surface Polymers on Multiwalled Carbon Nanotubes for Selective Extraction and Electrochemical Determination of Rhodamine B in Food Samples

by Yassine Benmassaoud, Khaled Murtada, Rachid Salghi, Mohammed Zougagh and Ángel Ríos

Molecules 2021, 26(9), 2670; https://doi.org/10.3390/molecules26092670 - 02 May 2021

Cited by 12 | Viewed by 2928

Abstract

In this study, we combine magnetic solid phase extraction (MSPE), with the screen-printed carbon electrode (SPCE) modified by a molecular imprinted polymer (MIP) for sensitive and selective extraction and electrochemical determination of Rhodamine B in food samples. A magnetic solid phase extraction (MSPE) was carried out using magnetic poly(styrene-co-divinylbenzene) (PS-DVB) and magnetic nanoparticles (MNPs) synthetized on the surface of multiwalled carbon nanotubes (MWCNTs). An MIP was prepared on the surface of MWCNTs in the presence of titanium oxide nanoparticles (TiO₂NPs) modifying the SPCE for the rapid electrochemical detection of Rhodamine B. The MIPs synthesis was optimized by varying the activated titanium oxide (TiO₂) and multiwalled carbon nanotubes (MWCNTs) amounts. The MSPE and electrochemical detection conditions were optimized as well. The present method exhibited good selectivity, high sensitivity, and good reproducibility towards the determination of Rhodamine B, making it a suitable method for the determination of Rhodamine B in food samples. Full article

(This article belongs to the Special Issue Nanomaterials Applied to Analytical Chemistry)

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Review

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45 pages, 4861 KiB

Open AccessReview

Covalent Organic Frameworks in Sample Preparation

by Javier González-Sálamo, Gabriel Jiménez-Skrzypek, Cecilia Ortega-Zamora, Miguel Ángel González-Curbelo and Javier Hernández-Borges

Molecules 2020, 25(14), 3288; https://doi.org/10.3390/molecules25143288 - 20 Jul 2020

Cited by 28 | Viewed by 5904

Abstract

Covalent organic frameworks (COFs) can be classified as emerging porous crystalline polymers with extremely high porosity and surface area size, and good thermal stability. These properties have awakened the interests of many areas, opening new horizons of research and applications. In the Analytical Chemistry field, COFs have found an important application in sample preparation approaches since their inherent properties clearly match, in a good number of cases, with the ideal characteristics of any extraction or clean-up sorbent. The review article is meant to provide a detailed overview of the different COFs that have been used up to now for sample preparation (i.e., solid-phase extraction in its most relevant operational modes—conventional, dispersive, magnetic/solid-phase microextraction and stir-bar sorptive extraction); the extraction devices/formats in which they have been applied; and their performances and suitability for this task. Full article

(This article belongs to the Special Issue Nanomaterials Applied to Analytical Chemistry)

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