Separation Techniques on a Miniaturized Scale

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Chromatographic Separations".

Deadline for manuscript submissions: 10 November 2025 | Viewed by 2180

Special Issue Editors


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Guest Editor
Institute of Chemistry of São Carlos, University of São Paulo, São Carlos 13566-590, Brazil
Interests: liquid chromatography; gas chromatography; supercritical fluid chromatography; capillary unified chromatography; electrophoresis; mass spectrometry; GC-MS(MS); LC-HRMS

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Guest Editor
São Carlos Institute of Chemistry, University of São Paulo, São Carlos 13566-590, Brazil
Interests: chromatography; mass spectrometry; sample preparation; HPLC; UPLC

Special Issue Information

Dear Colleagues,

Miniaturization has emerged as a promising frontier in separation science, offering unprecedented opportunities for enhancing separation processes' efficiency, sensitivity, and portability. With this in mind, this Special Issue explores the latest innovations and advancements in microscale separation sciences. All kinds of miniaturized techniques will be covered, from sample preparation micro techniques (SPME, SBSE, MEPS, SDME, DLLME, and HF-LPME), chromatographic techniques (capillary GC, capillary LC, and capillary SFC), electrophoretic techniques (CZE, EC, and c-ITP), integrated microfluidic systems for sample preparation and analysis, etc. Also, their coupling with other techniques such as mass spectrometry (cLC-MS, EC-MS, and SFC-MS) and multidimensional systems such as GC-GC, GCxGC, LC-LC, microLC-GC, microLC-SFC, and others will be included in this Special Issue. In addition to instrumentation, this Special Issue will comprise method development and application of the various miniaturized separation techniques to analyze food samples, pharmaceutical, environmental, drugs, fuels, OMICS, industrial, and samples relevant to other arenas. Therefore, we are pleased to invite you to contribute with your research article, communication, or review to this Special Issue entitled “Separation Techniques on a Miniaturized Scale”.

Prof. Dr. Fernando Lanças
Dr. Deyber Arley Vargas Medina
Guest Editors

Manuscript Submission Information

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Keywords

  • miniaturized sample preparation
  • sorbent-based microextraction
  • solvent-based microextraction
  • miniaturized instrumentation
  • green analytical chemistry
  • liquid chromatography
  • gas chromatography
  • open tubular liquid chromatography
  • capillary electrophoresis
  • microfluidic devices

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Published Papers (3 papers)

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Research

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20 pages, 1963 KiB  
Article
MEMS-Based Micropacked Thermal Desorption GC/PID for In-Field Volatile Organic Compound Profiling from Hot Mix Asphalt
by Stefano Dugheri, Giovanni Cappelli, Riccardo Gori, Stefano Zampolli, Niccolò Fanfani, Ettore Guerriero, Donato Squillaci, Ilaria Rapi, Lorenzo Venturini, Alexander Pittella, Chiara Vita, Fabio Cioni, Domenico Cipriano, Mieczyslaw Sajewicz, Ivan Elmi, Luca Masini, Simone De Sio, Antonio Baldassarre, Veronica Traversini and Nicola Mucci
Separations 2025, 12(5), 133; https://doi.org/10.3390/separations12050133 - 19 May 2025
Abstract
Background: In response to the growing demand for the real-time, in-field characterization of odorous anthropogenic emissions, this study develops and uses a MEMS-based micropacked thermal desorption Gas Chromatography system coupled with a PhotoIonization Detector (GC/PID) for Hot Mix Asphalt (HMA) plant emissions. Methods: [...] Read more.
Background: In response to the growing demand for the real-time, in-field characterization of odorous anthropogenic emissions, this study develops and uses a MEMS-based micropacked thermal desorption Gas Chromatography system coupled with a PhotoIonization Detector (GC/PID) for Hot Mix Asphalt (HMA) plant emissions. Methods: The innovative portable device, Pyxis GC, enables the high-sensitivity profiling of Volatile Organic Compounds (VOCs), particularly aldehydes and ketones, with sub-ppb detection limits using ambient air as the carrier gas. A comprehensive experimental design optimized the preconcentration parameters, resulting in an efficient, green analytical method evaluated via the Green Analytical Procedure Index (GAPI). Sorbent comparison showed quinoxaline-bridged cavitands outperform the conventional materials. Results and conclusions: The method was successfully deployed on site for source-specific sampling at an HMA plant, generating robust emission fingerprints. To assess environmental impact, a Generalized Additive Model (GAM) was developed, incorporating the process temperature and Sum of Odour Activity Values (SOAV) to predict odour concentrations. The model revealed a significant non-linear influence of temperature on emissions and validated its predictive capability despite the limited sample size. This integrated analytical–statistical approach demonstrates the utility of MEMS technology for real-time air quality assessment and odour dispersion modelling, offering a powerful tool for environmental monitoring and regulatory compliance. Full article
(This article belongs to the Special Issue Separation Techniques on a Miniaturized Scale)
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17 pages, 5353 KiB  
Article
A Compact Instrument for Temperature-Programming-Assisted Capillary–Nanoliquid Chromatography
by Lincon Coutinho Marins, Alessandra Maffei Monteiro, Vivane Lopes Leal, Deyber Arley Vargas Medina, Edwin Martin Cardenas and Fernando Mauro Lanças
Separations 2025, 12(1), 5; https://doi.org/10.3390/separations12010005 - 30 Dec 2024
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Abstract
The miniaturization of liquid chromatography (LC) columns to capillary and nanoscales allows temperature programming to be an effective alternative to solvent gradients for modulating eluotropic strength. This approach simplifies instrument design and operation, as a single pump can suffice to achieve efficient separations. [...] Read more.
The miniaturization of liquid chromatography (LC) columns to capillary and nanoscales allows temperature programming to be an effective alternative to solvent gradients for modulating eluotropic strength. This approach simplifies instrument design and operation, as a single pump can suffice to achieve efficient separations. This study presents the development and application of a compact, lab-built high-pressure system for temperature-programmed capillary and nanoLC separations. The instrument includes a high-pressure capillary–nanoflow syringe pump, a time-based nanoliter injection system, a programmable capillary column oven for controlled temperature gradients, and a UV-Vis detection system with a custom nanoliter-scale detection cell. Each system component was designed and built in-house, with rigorous calibration to ensure accuracy and operational reliability. Experimental data confirm the system’s capability to deliver precise, reproducible temperature, and flow rates. Functionality was validated through temperature-programmed separations on packed and open tubular capillary columns. The results demonstrated that the developed instrument offers enhanced separation efficiency and reduced analysis time compared to isothermal methods, underscoring its potential for advanced applications in miniaturized liquid chromatography. Full article
(This article belongs to the Special Issue Separation Techniques on a Miniaturized Scale)
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Review

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30 pages, 2179 KiB  
Review
Advancements in Microextraction by Packed Sorbent: Insights into Sorbent Phases and Automation Strategies
by Rafael Oliveira Martins, João Victor Basolli Borsatto, Camila Will and Fernando Mauro Lanças
Separations 2025, 12(1), 11; https://doi.org/10.3390/separations12010011 - 8 Jan 2025
Viewed by 1022
Abstract
Miniaturized solid-based approaches have added an eco-friendly dimension to analytical procedures, establishing themselves as promising strategies for a wide range of applications. Among these, microextraction by packed sorbent (MEPS) stands out due to its ability to facilitate efficient sample interaction with a densely [...] Read more.
Miniaturized solid-based approaches have added an eco-friendly dimension to analytical procedures, establishing themselves as promising strategies for a wide range of applications. Among these, microextraction by packed sorbent (MEPS) stands out due to its ability to facilitate efficient sample interaction with a densely packed sorb ent phase within the microextraction system. MEPS offers several advantages, including preconcentration capabilities and the use of minimal sample and solvent volumes, making it an appealing choice for modern analytical workflows. Since the extraction efficiency is largely dictated by the sorbent phase, recent advancements in sorbent design have garnered considerable attention in the field of sample preparation. Innovations in sorbent phases have not only enhanced the MEPS efficiency but also enabled the development of semi- and fully automated systems, paving the way for high-throughput methodologies. These advancements have elevated MEPS beyond traditional offline miniaturized sample preparation methods, offering new opportunities for streamlined and scalable analyses. Therefore, this study provides a comprehensive overview of novel sorbent phases used in MEPS, with a particular focus on both bio-based and synthetic materials. Furthermore, it explores the semi- and fully automated aspects of MEPS, highlighting current trends, technological advancements, and future directions in this rapidly evolving field. Full article
(This article belongs to the Special Issue Separation Techniques on a Miniaturized Scale)
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